CN102845455A - High-efficient cyhalothrin microcapsule suspending agent and preparation method thereof - Google Patents
High-efficient cyhalothrin microcapsule suspending agent and preparation method thereof Download PDFInfo
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- CN102845455A CN102845455A CN2012100868585A CN201210086858A CN102845455A CN 102845455 A CN102845455 A CN 102845455A CN 2012100868585 A CN2012100868585 A CN 2012100868585A CN 201210086858 A CN201210086858 A CN 201210086858A CN 102845455 A CN102845455 A CN 102845455A
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Abstract
The invention discloses a high-efficient cyhalothrin microcapsule suspending agent and a preparation method thereof; the suspending agent comprises the following components by weight: 1%-10% of high-efficient cyhalothrin, 3%-20% of a capsule core solvent, 5%-30% of a capsule wall material, 3%-10% of an emulsifier, 1%-5% of a dispersant, 0.1%-10% of a pH adjusting agent, and the balance of deionized water. The invention also discloses the preparation method of the high-efficient cyhalothrin microcapsule suspending agent. The product of the invention is low in cost, stable in performance, good in insecticidal effect, long in persistent period, low in toxicity, friendly to environment, and safe for people and livestock, and can meet the requirements of insect pollution-free control.
Description
Technical field
The present invention relates to a kind of agricultural insecticide and preparation method thereof, specifically a kind of gamma cyhalothrin micro-capsule suspension and preparation method thereof.
Background technology
Chemical control is the important means of control agricultural damage by disease and insect, chemical pesticide plays very important effect to the increasing both production and income that guarantees agricultural, yet the use of agricultural chemicals when Ensuring Food Safety is produced, has also brought a series of environment and the social concerns such as residual, pollution.Be not only because chemical pesticide itself, and be because the formulations of pesticide are processed and application process is unreasonable causes to a great extent.It is reported, the availability of regular dosage form agricultural chemicals only has 20%~30%, and percent of loss by all means is up to 50%~60%, and this not only is a kind of waste economically, and has caused large-scale environmental pollution.Therefore, develop safety, high-efficiency environment friendly, prolongation lasting period, alleviate poisoning, reduce the novel form preparation residual, that increase the range of application of agricultural chemicals of agricultural chemicals in environment and become one of developing direction of pesticide in future formulation.
The pesticide micro capsule suspending agent is to utilize the capsule-core that microencapsulation technology will contain former medicine to be encapsulated in the suspending agent that forms fine particle in the special cyst material, and the capsule diameter of agricultural chemicals microcapsule suspending agent is generally 1~20 μ m.The agricultural chemicals microcapsule suspending agent is compared with conventional dosage forms and is had the following advantages: prolonged the lasting period of agricultural chemicals, the stability that has improved active component, active substance be wrapped in improved in the cyst wall safety, effectively reduce former medicine composition to the stimulus to the sense organ of human body, reduce poisoning to crop, be conducive to the composite, more friendly to environment of agricultural chemicals.
Gamma cyhalothrin claims again Cyhalothrin, cyhalothrin, belongs to intending the worm chrysanthemum ester insecticide, has and tags and stomach poison function, and insect and mite are had strong tagging and stomach poison function, and certain repellent action is also arranged.Have very high biologically active, insecticidal spectrum is wide, and is effective to Lepidoptera, coleoptera, Semiptera, thrips, Hymenoptera, orthoptera, dipterous various pests, and insecticidal action is fast, low to the toxicity of natural enemy.But the duration of the cyhalothrin pest control that uses at present is too short, causes the frequent medication of peasant and improves constantly dosing, and many areas have all caused drug-fast generation, and the lasting period that for this reason prolongs this medicament becomes the problem that needs to be resolved hurrily.In addition, the formulation that gamma cyhalothrin uses at present owing to using a large amount of organic solvents, not only consumes a large amount of petrochemical industry resources still take missible oil as main, and environment has also been caused very large pressure.Therefore, the environment friendly agricultural preparation that research and development are good with Environmental compatibility both can be brought into play its effectiveness to greatest extent, prolonged its operating period, overcame pesticide resistance, can save substantial contribution and labour again.
Summary of the invention
The purpose of this invention is to provide a kind of gamma cyhalothrin micro-capsule suspension, can prolong the lasting period, overcome pest resistance to insecticide, little to environmental pressure, economize on resources, be conducive to the sustainable development of agricultural and the protection of environment.
Another object of the present invention provides a kind of preparation method of above-mentioned gamma cyhalothrin micro-capsule suspension.
The present invention is achieved by the following technical solutions: a kind of gamma cyhalothrin micro-capsule suspension, component by following percentage by weight forms: gamma cyhalothrin 1%~10%, capsule-core solvent 3%~20%, cyst material 5%~30%, emulsifier 3%~10%, dispersant 1%~5%, pH adjusting agent 0.1%~10%, surplus are deionized water.
Wherein said capsule-core solvent is one or more among dimethylbenzene, cyclohexanone, ethyl acetate, 1-METHYLPYRROLIDONE, diethyl phthalate, dibutyl phthalate, Solvesso100, Solvesso150, the Solvesso200.
Described cyst material is the urea resin prepolymer aqueous solution, is to be mixed with weight ratio 1:1~1:2.5 by urea and formaldehyde, obtains by polycondensation reaction.
Described emulsifier is one or more in alkylphenol polyoxyethylene, styryl phenol polyethenoxy ether, alkaryl phenol polyethenoxy ether phosphate, castor oil polyoxyethylene ether, alkylbenzenesulfonate, alkylphenol-polyethenoxy phosphate, disecoctylmaleate sodium sulfonate, polyol fatty acid ester and the ethylene oxide adduct thereof.
Described dispersant is one or more in SOPA-270, dispersant NNO, sodium lignin sulfonate, the dispersant 2700.
Described pH adjusting agent is sodium hydroxide or watery hydrochloric acid.
A kind of preparation method of gamma cyhalothrin micro-capsule suspension is as follows.
(1) urea is dissolved in the formaldehyde, the weight ratio that urea and formaldehyde mix is 1:1~1:2.5, regulating the pH value with sodium hydroxide is 8~9, under 60~80 ℃ of conditions of temperature, stirring at low speed, insulation reaction 0.5~4 hour, generate the transparent Lauxite of thickness, the deionized water that adding equates with urea and formaldehyde gross weight, stirring at low speed obtains the transparent urea resin prepolymer aqueous solution.
(2) at normal temperatures gamma cyhalothrin is dissolved in the capsule-core solvent fully, when stirring, adds a certain amount of urea resin prepolymer aqueous solution, with 1000~2000 rev/mins of rotating speed cutting 10~20 minutes, obtain stable O/W emulsion.
(3) reduce the rotating speed of shearing, adding in batches watery hydrochloric acid and regulate the pH value in 1 hour is 2.0, polycondensation reaction occurs, progressively be warming up to 40~60 ℃ and solidify cyst wall, reacting after 1.5~2 hours cyst wall solidifies and finishes, add sodium hydroxide again and regulate pH value to 6.0~7.0, add an amount of emulsifier, dispersant, deionized water complements to 100%.With 2000~6000 rev/mins of rotating speed high shears 10~60 minutes, namely obtain the gamma cyhalothrin micro-capsule suspension again.
In the cyst wall solidify reaction process, every sampling in 15 minutes 1 time, use the capsule process of each stage of reaction of microscopic examination, use the pH value of pH meter monitoring reaction course.
Advantage of the present invention and good effect are as follows.
1, gamma cyhalothrin micro-capsule suspension provided by the invention, flash-point is high, does not burn and does not explode, and produces and stores and use safety.
2, gamma cyhalothrin micro-capsule suspension provided by the invention, farm chemical ingredients slowly discharges after the dispenser, can a dispenser protect one season of effect, saves medicament, saves man-hour.
3, gamma cyhalothrin micro-capsule suspension provided by the invention, contact toxicity and peculiar smell reduce greatly, make the operator avoid harm.
4, gamma cyhalothrin micro-capsule suspension provided by the invention, consumption of organic solvent reduces more than 30%, has greatly reduced harmful aromatic hydrocarbons to the pollution of environment, is conducive to environmental protection.
5, gamma cyhalothrin micro-capsule suspension provided by the invention, product cost is low, stable performance, good disinsection effect, the lasting period is long, and low toxicity is environmentally friendly, to the person poultry safety, can satisfy the non-environmental pollution control needs of insect.
6, the preparation method of invention easily operates.
Embodiment
Essence for a better understanding of the present invention, the below illustrates technology contents of the present invention with embodiment, but content of the present invention is not limited to this.
According to the preparation method who the invention provides a kind of gamma cyhalothrin micro-capsule suspension, can make the gamma cyhalothrin percentage by weight and be 1%~10% micro-capsule suspension.
Embodiment 1:2% gamma cyhalothrin micro-capsule suspension.
Urea resin prepolymer water solution preparation method: urea is dissolved in the formaldehyde, the weight ratio that urea and formaldehyde mix is 1:2.5, regulating the pH value with sodium hydroxide is 8, under the temperature 60 C condition, stirring at low speed, insulation reaction 0.5 hour, generate the transparent Lauxite of thickness, the deionized water that adding equates with urea and formaldehyde gross weight, stirring at low speed obtains the transparent urea resin prepolymer aqueous solution.
At normal temperatures 2% gamma cyhalothrin is dissolved in 5% dimethylbenzene fully, adds while stirring the 10% urea resin prepolymer aqueous solution, with 2000 rev/mins of rotating speed cutting 10 minutes, obtain stable O/W emulsion.Reduce rotating speed to 1000 rev/min, minutes 5 batches added watery hydrochloric acid to regulate the pH value are 2.0 in 1 hour, polycondensation reaction occurs, progressively be warming up to 45 ℃ and solidified cyst wall 1.5 hours, add again sodium hydroxide and regulate pH value to 6.5, add emulsifier alkylphenol polyoxyethylene 4%, alkylbenzenesulfonate 1.5%, dispersant SOPA-2700 1.5%, complement to 100% with deionized water.With 4000 rev/mins of rotating speed high shears 15 minutes, namely obtain 2% gamma cyhalothrin micro-capsule suspension again.
Embodiment 2:5% gamma cyhalothrin micro-capsule suspension.
Urea resin prepolymer water solution preparation method: urea is dissolved in the formaldehyde, the weight ratio that urea and formaldehyde mix is 1:2, regulating the pH value with sodium hydroxide is 9, under 80 ℃ of conditions of temperature, stirring at low speed, insulation reaction 4 hours, generate the transparent Lauxite of thickness, the deionized water that adding equates with urea and formaldehyde gross weight, stirring at low speed obtains the transparent urea resin prepolymer aqueous solution.
At normal temperatures 5% gamma cyhalothrin is dissolved in 12% dimethylbenzene fully, adds while stirring the 25% urea resin prepolymer aqueous solution, with 1500 rev/mins of rotating speed cutting 20 minutes, obtain stable O/W emulsion.Reduce rotating speed to 800 rev/min, minutes 5 batches added watery hydrochloric acid to regulate the pH value are 2.0 in 1 hour, polycondensation reaction occurs, progressively be warming up to 50 ℃ and solidified cyst wall 1.5 hours, add again sodium hydroxide and regulate pH value to 6.5, add emulsifier castor oil polyoxyethylene ether 3%, disecoctylmaleate sodium sulfonate 4%, alkylbenzenesulfonate 1.5%, dispersant NNO 1%, complement to 100% with deionized water.With 5000 rev/mins of rotating speed high shears 15 minutes, namely obtain 5% gamma cyhalothrin micro-capsule suspension again.
Gamma cyhalothrin micro-capsule suspension properties of product of the present invention are stable, are easy to produce store, and are environmentally friendly, to the person poultry safety.Through evidence, to the various pests such as Lepidoptera, coleoptera and Semiptera of wheat, corn, cotton and multiple fruit tree and vegetable, and the evil mite such as tetranychid, rust mite, goitre mite all has good result; Safety is good, to crops without poisoning.
Claims (2)
1. gamma cyhalothrin micro-capsule suspension, it is characterized in that: described micro-capsule suspension is comprised of the component of following percentage by weight: gamma cyhalothrin 1%~10%, capsule-core solvent 3%~20%, cyst material 5%~30%, emulsifier 3%~10%, dispersant 1%~5%, pH adjusting agent 0.1%~10%, surplus are deionized water;
Wherein said capsule-core solvent is one or more among dimethylbenzene, cyclohexanone, ethyl acetate, 1-METHYLPYRROLIDONE, diethyl phthalate, dibutyl phthalate, Solvesso100, Solvesso150, the Solvesso200;
Described cyst material is the urea resin prepolymer aqueous solution, is to be mixed with weight ratio 1:1~1:2.5 by urea and formaldehyde, obtains by polycondensation reaction;
Described emulsifier is one or more in alkylphenol polyoxyethylene, styryl phenol polyethenoxy ether, alkaryl phenol polyethenoxy ether phosphate, castor oil polyoxyethylene ether, alkylbenzenesulfonate, alkylphenol-polyethenoxy phosphate, disecoctylmaleate sodium sulfonate, polyol fatty acid ester and the ethylene oxide adduct thereof;
Described dispersant is one or more in SOPA-270, dispersant NNO, sodium lignin sulfonate, the dispersant 2700;
Described pH adjusting agent is sodium hydroxide or watery hydrochloric acid.
2. the preparation method of a gamma cyhalothrin micro-capsule suspension is characterized in that:
(1) urea is dissolved in the formaldehyde, the weight ratio that urea and formaldehyde mix is 1:1~1:2.5, regulating the pH value with sodium hydroxide is 8~9, under 60~80 ℃ of conditions of temperature, stirring at low speed, insulation reaction 0.5~4 hour, generate the transparent Lauxite of thickness, the deionized water that adding equates with urea and formaldehyde gross weight, stirring at low speed obtains the transparent urea resin prepolymer aqueous solution;
(2) at normal temperatures gamma cyhalothrin is dissolved in the capsule-core solvent fully, when stirring, adds a certain amount of urea resin prepolymer aqueous solution, with 1000~2000 rev/mins of rotating speed cutting 10~20 minutes, obtain stable O/W emulsion;
(3) reduce the rotating speed of shearing, adding in batches watery hydrochloric acid and regulate the pH value in 1 hour is 2.0, polycondensation reaction occurs, progressively be warming up to 40~60 ℃ and solidify cyst wall, reacting after 1.5~2 hours cyst wall solidifies and finishes, add sodium hydroxide again and regulate pH value to 6.0~7.0, add an amount of emulsifier, dispersant, deionized water complements to 100%;
With 2000~6000 rev/mins of rotating speed high shears 10~60 minutes, namely obtain the gamma cyhalothrin micro-capsule suspension again;
In the cyst wall solidify reaction process, every sampling in 15 minutes 1 time, use the capsule process of each stage of reaction of microscopic examination, use the pH value of pH meter monitoring reaction course.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103329897A (en) * | 2013-07-10 | 2013-10-02 | 中国科学院新疆生态与地理研究所 | Pyrethroid insecticide controlled-release polymer microcapsule synthesis method |
CN105076191A (en) * | 2015-08-20 | 2015-11-25 | 广东中迅农科股份有限公司 | Efficient cyfluthrin microcapsule suspending agent and preparation method thereof |
CN105076202A (en) * | 2015-08-27 | 2015-11-25 | 广东中迅农科股份有限公司 | Microcapsule suspension containing fosthiazate and beta-cyfluthrin |
CN106386800A (en) * | 2016-08-31 | 2017-02-15 | 北京明德立达农业科技有限公司 | Preparation method of cyhalothrin and chlorfluazuron microcapsule suspension-suspension and microcapsule suspension-suspension |
CN106634281A (en) * | 2016-12-27 | 2017-05-10 | 重庆市风景园林科学研究院 | Novel environmental-friendly transparent trunk coating for trees and preparation method of trunk coating |
CN107691444A (en) * | 2017-09-20 | 2018-02-16 | 江苏明德立达作物科技有限公司 | A kind of Fenpropathrin microcapsule suspending agent and preparation method thereof |
CN108477201A (en) * | 2018-05-16 | 2018-09-04 | 安徽省四达农药化工有限公司 | A kind of gamma cyhalothrin micro-capsule suspension and preparation method thereof |
CN109953021A (en) * | 2017-12-26 | 2019-07-02 | 华东理工大学 | Pyrethroids microcapsules, preparation method and insect prevention preparation |
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CN1792157A (en) * | 2005-12-30 | 2006-06-28 | 山东农业大学 | High performance cypermethrin micro-capsule emulsion |
CN101731210A (en) * | 2008-11-05 | 2010-06-16 | 河北农业大学 | Process for preparing pesticide microcapsules by interfacial polymerization method |
CN101811014A (en) * | 2010-04-01 | 2010-08-25 | 西安科技大学 | Method for preparing microcapsule |
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Patent Citations (3)
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CN1792157A (en) * | 2005-12-30 | 2006-06-28 | 山东农业大学 | High performance cypermethrin micro-capsule emulsion |
CN101731210A (en) * | 2008-11-05 | 2010-06-16 | 河北农业大学 | Process for preparing pesticide microcapsules by interfacial polymerization method |
CN101811014A (en) * | 2010-04-01 | 2010-08-25 | 西安科技大学 | Method for preparing microcapsule |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103329897A (en) * | 2013-07-10 | 2013-10-02 | 中国科学院新疆生态与地理研究所 | Pyrethroid insecticide controlled-release polymer microcapsule synthesis method |
CN105076191A (en) * | 2015-08-20 | 2015-11-25 | 广东中迅农科股份有限公司 | Efficient cyfluthrin microcapsule suspending agent and preparation method thereof |
CN105076202A (en) * | 2015-08-27 | 2015-11-25 | 广东中迅农科股份有限公司 | Microcapsule suspension containing fosthiazate and beta-cyfluthrin |
CN106386800A (en) * | 2016-08-31 | 2017-02-15 | 北京明德立达农业科技有限公司 | Preparation method of cyhalothrin and chlorfluazuron microcapsule suspension-suspension and microcapsule suspension-suspension |
CN106634281A (en) * | 2016-12-27 | 2017-05-10 | 重庆市风景园林科学研究院 | Novel environmental-friendly transparent trunk coating for trees and preparation method of trunk coating |
CN107691444A (en) * | 2017-09-20 | 2018-02-16 | 江苏明德立达作物科技有限公司 | A kind of Fenpropathrin microcapsule suspending agent and preparation method thereof |
CN109953021A (en) * | 2017-12-26 | 2019-07-02 | 华东理工大学 | Pyrethroids microcapsules, preparation method and insect prevention preparation |
CN108477201A (en) * | 2018-05-16 | 2018-09-04 | 安徽省四达农药化工有限公司 | A kind of gamma cyhalothrin micro-capsule suspension and preparation method thereof |
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